Process of obtaining ceresin and the like from residues of mineral oil.



No Drawing.

JANMIJS, or BUssuM, NETHERLANDS.

PROCESS OF OBTAINING CER-ESIN AND THE LIIIIKE FROM RESIDUES F MINERALOIL.

T 0 all whom it mag concern Be it known that I, JAN Mus, a sub e ct I ofthe Queen of the Netherlands, residing 1n Bussum, Netherlands, (whosepost-ofiice address is Villa Omega,. Nieuwes Gravelandsche Weg -57,Bussum, Netherlands,)

chemist, have invented a certain new and useful Process of ObtainingCeresin and the like from Residues of Mineral Oil,'of which.

the following is a specification.

The present invention relates to a process of obtaining ceresin orpurified ozocerite and other solid "hydrocarbons of known kind, such asparafiins, from mineral oil residues, that is to say, the substanceremaining in the still after the several fractions up to and includinglubricating oils have been distilled from crude petroleum, and from themore or less soiled substance obtained during purification of variouscrude petroleum .distillates with sulfuric acid and the mineral oils ofbuttery consistency found in Russia, Roumania, India, and elsewhere. Theuse for such purposes of b'enzin, acetic ether or homologous esters,carbon or other halogen substitution products of saturatedandnon--saturated hydrocarbons is well known, acetic acid (glacial fectsattend the use of such solvents.

acetic acid), propi'onic acid, butyric acid or the like being preferablyadded. Great de- Tetrachlorid of carbon in particular, as Well as othercompounds {containing chlorin, and also acid compounds (glacial aceticacid-or the like) damage the apparatus, attacking the metal parts sothat expensive apparatus protected in a special manner from such attackmust be used. Moreover, tetrachlorid I of carbon and benzin have verylow boiling points and'when working with such readily volatile liquidsgreat losses are unavoidable. Chlorin compounds such as tetrachlorid ofcarbon have an injurious action on the health of the persons workingwith them. The process constituting the subject-matter of the presentinvention obivates these defects' by using toluene, or more strictlyspeaking toluol having. a boiling point of 110 degrees (1., instead ofthe solvents hitherto used. This solvent is, firstly, relativelyinexpensive, secondly, can be readily obtained in large quantities to beconsidered when working with this solvent. Furthermore, the toluene,having Specification of Letters Patent.

tetrachlorid of r and, thirdly, is v specially distinguished by a highboiling "point, so that appreciable losses hardly have Patented Apr. 11,1916.

Application filed May 11, 1912. Serial No. 696,707.

boiling point of 110 degrees (1., can by distillation be recoveredcomparatively simply and almost without loss.

The applicant is Well aware that he is not the first to propose the useof toluol in preference to benzol as a solvent of paraffin, but he isthe first to discover that ceresin, p'araflin and other solidhydrocarbons from mineral-oil residues, instead of being precipitatedinjelly-like or colloidal form as they would be on cooling from benzolsolutions will, when the residues are treated with toluol having thespecified boiling point, or in other words with toluene, be

precipitated in a more crystalline form.

Thereconsequently issues from his discovery the fact that toluene isbetter suited than the solvents heretoforeused, for obtaining from theresidues in question solid hydrocarbons in excellent yield and ofexcellent nature.

The following example will serve to show how my process may be carriedinto practice in obtaining purified ozocerite or ceresin: The residuesreferred to in the opening'paragraph of this specification andpreferably preliminarily purified in the usual manner by mixing themwith a proper proportion of sulfuric acid and subsequently neutralizingthem, are intimately mixed in closed mixers of ordinaryconstruction-with approximately an equal quantity of toluene heated toabout 50-80 C., but the exact amount of toluene to be added depends, in

general, on the composition of the residues. After agitating theresidues for an appropriate period, for instance, about twenty minutes,with the toluene, the toluene solut1on, perature within the abovelimits, is allowed to cool to a temperature which is dependent on themelting point of the product to be obtained and may vary from 25 degreesto 60 degrees C., and the undissolved'constituents are separated out inany suitable known manner, for example by filter presses. The separatedcrude ozocerite substance is further purified by means of, first,sulfuric acid solution, as explained above, and then by magnesiahydrosilicate (fullers earth). The ceresin or ozocerite; obtained inthis which has been maintained at a tem-.

manner is of a better quality than the products obtained accor'dingvtowell-known processes. Particularly, the ceresin has a higher meltingpoint and is not so sticky as that obtained 1n the manner knownheretofore from the same mineral-oil residue. Lastly, the

yield of this ceresin of a. higher melting point is likewise greater.The separated solution can be at first cooled, to say 50 degrees (1.,toobtain the hydrocarbons with .high melting point and then be cooledfurther, to say, 30 degrees (1., whereupon the hydrocarbons, with lowermelting point, can

be obtained. Lastly, almost all the toluene can be recovered. Theresidue which is then left can be used for various technical purposes.The procedure is the same whether mineral oil residues or mineral tarsare un der treatment, except that the more solid the material the largerthe proportion of toluene used.

Other solid hydrocarbons, such as paraflin and the like, can also beobtained from other mineral oil residues, for example, shale oilresidues, in like manner as ceresin or puri fied ozocerite fromozocerite residues.

Having now described the nature of my said mvention and the best means Iknow of carrying the same into practical efiect, I;

claim 1. A process of obtaining in a crystalline form ceresin (purifiedozocerite), paraflin and other solid hydrocarbons from mineralconsistsin first subjecting the residues to a preliminary purification, thenmixing the same in closed mixers with approximately an equal quantity'oftoluene, having a boiling point of 110 degrees (1., andat a temperature.in excess ofrfifty degrees C., and

then separating the toluene from the undissolved solid matterbefore itis cooled. I

- In-testimony whereof I have signed my name to this specification inthe presence of two subscribing Witnesses. y

m JANMIJS. Witnesses-z v JOSEPH MILLARI),

W. I. S. MERTEN."

